药用辅料聚乙二醇6000中醛类测定方法的比较研究  

The Comparative Study of Methods for Determination of Aldehydes in Pharmaceutical Excipient Polyethylene Glycol 6000

作　　者：石蓉 谢莹莹 郑金凤 张悦 尹林高 刘雁鸣 SHI Rong;XIE Yingying;ZHENG Jinfeng;ZHANG Yue;YIN Lingao;LIU Yanming(Hunan Institute for Drug Control,NMPA Key Laboratory for Pharmaceutical Excipients Engineering Technology Research,Changsha Hunan 410001,China;Hunan Drug Inspection Center,Changsha Hunan 410001,China)

机构地区：[1]湖南省药品检验检测研究院,国家药品监督管理局药用辅料工程技术研究重点实验室,湖南长沙410001 [2]湖南省药品审核查验中心,湖南长沙410001

出　　处：《药品评价》2023年第9期1090-1095,共6页Drug Evaluation

基　　金：湖南省食品药品监督管理局食品药品安全科技项目(2021JJ80044)。

摘　　要：目的 探寻药用辅料聚乙二醇6000最有效的醛类控制方法,为其质量标准制修订提供参考和依据。方法 采用法定标准变色酸法测定聚乙二醇6000中甲醛含量,建立DNPH柱前衍生-高效液相色谱法测定聚乙二醇6000中甲醛、乙醛含量,采用酚试剂法测定聚乙二醇6000中总醛含量,并对样品测定结果进行比较。结果 法定标准变色酸法易受样品干扰,影响显色,造成甲醛测定结果低于实际含量;建立的DNPH柱前衍生-高效液相色谱法检出限低,方法准确度和重复性均良好;酚试剂法操作简便,可用于聚乙二醇6000中总醛含量测定。结论 DNPH柱前衍生-HPLC法可以用于聚乙二醇6000的甲醛、乙醛定量分析,结合酚试剂测定总醛含量,可以从总体上控制聚乙二醇6000的醛类物质。Objective To explore the most effective aldehydes control method for pharmaceutical excipients polyethylene glycol 6000,and provide reference and basis for the revision of its quality standard.Methods The content of formaldehyde in polyethylene glycol 6000 was determined by the chromotropic acid method listed in the statutory standard,the content of formaldehyde and acetaldehyde in polyethylene glycol 6000 were determined by high performance liquid chromatography with DNPH pre-column derivatization,and the content of total aldehyde in polyethylene glycol 6000 was determined by phenol reagent method,all results of sample determination by three methods were compared.Results The discoloration acid method listed in the statutory standard was easy to be interfered by the sample,which affects the color development,resulting in the formaldehyde determination results lower than the actual content;the established method with DNPH pre-column derivation by HPLC had low detection limit,good accuracy and repeatability;the phenol reagent method was simple and can be used for the determination of total aldehyde content in polyethylene glycol 6000.Conclusion It can be used to control the aldehydes of PEG 6000 by the HPLC method with DNPH pre-column derivation which can be used for the quantitative analysis of formaldehyde and acetaldehyde and combining with phenol reagent method which can determine the total aldehyde content.

关 键 词：聚乙二醇6000 变色酸法 DNPH柱前衍生-高效液相色谱法 酚试剂法 甲醛 乙醛 总醛 

分 类 号：R917[医药卫生—药物分析学]